INORGANIC   CHEMICAL 
PREPARATIONS 


INORGANIC  CHEMICAL 
PREPARATIONS 


BY 


FELIX   LENGFELD 

ASSISTANT  PROFESSOR  OF  INORGANIC  CHEMISTRY  IN  THE 
UNIVERSITY  OF  CHICAGO 


THE   MACMILLAN   COMPANY 

LONDON  :  MACMILLAN  &  CO.,  LTD. 
I9II 

All  rights  reserved 


V 


7- 


COPYRIGHT,  1899, 
BY  THE  MACMILLAN  COMPANY. 

Setupandelectrotyped.     Published  August,  1899.     Reprinted 
December,  1905  ;  February,  19". 


J.  S.  Cashing  &  Co.  — Berwick  &  Smith  Co. 
Norwood,  Mass.,  U.S.A. 


PREFACE 

THIS  manual  was  written  for  the  classes 
in  Inorganic  Preparations  at  the  University 
of  Chicago.  The  course  is  intended  to 
familiarize  advanced  students  with  the 
methods  and  processes  used  in  making 
inorganic  compounds,  and  serves  at  the 
same  time  as  a  review  in  General  Chemis- 
try. It  is  supposed  that  the  student  who 
has  finished  the  course  is  able  without  fur- 
ther assistance  from  an  instructor  to  make 
any  inorganic  preparation.  An  attempt 
has  been  made  to  introduce  all  processes 
generally  used,  and  at  the  same  time  to 
avoid  repetition.  The  student  should  study 
each  preparation  in  detail,  work  out  other 
methods  of  making  the  same  substance, 

364848 


vi  PREFACE 

understand  and  criticise  every  step  he 
takes  and  read  some  original  articles. 
Therefore  references  to  the  literature  have 
been  given.  No  attempt  has  been  made 
to  make  the  list  of  references  complete,  as 
the  student  should  learn  to  use  dictiona- 
ries of  chemistry,  such  as  Dammer,  Graham- 
Otto,  etc. 

The  instructor  must  remember  that  the 
Manual  is  merely  a  laboratory  guide,  and 
that  unless  the  work  is  carefully  supervised 
it  may  become  purely  mechanical  and  the 
course  lose  half  its  value. 

The  preparations  have  not  been  arranged 
alphabetically  or  according  to  composition, 
but  rather  in  the  order  of  increasing  dif- 
ficulty. The  methods  have  all  been  tried 
and  have  been  found  to  give  good  results 
in  the  hands  of  careful  students.  A  table 
of  solubilities  is  appended. 


TABLE   OF  CONTENTS 

PAGE 

GENERAL  DIRECTIONS xi 

PREPARATIONS  : 

Sodium  Chloride I 

Potassium  Chlorate 2 

Bicarbonate  of  Soda       ......         3 

Sodium  Nitrite 4 

Basic  Lead  Nitrite 5 

Cuprous  Chloride 6 

Lead  Dioxide 7 

Mercuric  Oxide 8 

Boric  Acid 9 

Boron 10 

Sodium  Thiosulphate n   f- 

Barium  Dithionate          .         .         .         .         .         .12 

Ammonium  Nitrate         .         .         .         .         .         .13 

Sodium  Ammonium  Phosphate       .         .         .         -13 
Zinc  free  from  Arsenic    .        .         .         .         .         .14 

Arsenic  Acid  .         .         .         .         .         .         .       15 

Chrome  Alum         ....       >.         .         ,       15 


vm  TABLE  OF  CONTENTS 

PAGE 

PREPARATIONS  : 

Chromic  Anhydride 16 

Chromous  Acetate 17 

Hydrobromic  Acid 18 

Hydriodic  Acid 19 

Tin  Tetrachloride 21 

Sulphuryl  Chloride 22 

Phosphorus  Trichloride 23 

Fluorsilicic  Acid 25 

Antimony  Trichloride 25 

Antimony  Oxychloride 27 

Silver  Nitrate 27 

Silver  Hyponitrite 29 

Strontium  Chloride 30 

Strontium  Hydroxide 30 

Manganous  Chloride 31 

Manganese 31 

Iodine  Trichloride 33 

lodic  Acid 34 

Potassium  Fluortitanate 34 

Titanic  Oxide 35 

Sulphur  Monobromide 35 

Nitrogen  Iodide 36 

Nitrogen  Tetroxide 36 

Nitric  Anhydride 37 


TABLE  OF  CONTENTS  ix 

PAGE 

PREPARATIONS  : 

Sulphuric  Anhydride 39 

Aluminium  Chloride 40 

Potassium  Permanganate 41 

Crystallized  Silicon 42 

Silicochloroform 43 

Hydrogen  Persulphide 45 

Barium  Oxide 46 

Hydrated  Barium  Peroxide 47 

Hydrogen  Dioxide          ......  48 

Hydroxylamine  Sulphate 49 

Phosphonium  Iodide 51 

TABLE  OF  SOLUBILITIES 54 

INDEX  . 57 


GENERAL   DIRECTIONS 

A  GAS  should  always  be  washed  unless 
there  is  specific  reason  for  not  doing  so. 
If  the  gas  is  very  soluble  in  water,  and 
washing  would  involve  too  much  loss,  it 
may  frequently  be  purified  by  passing  it 
into  a  litre  bottle  before  using  so  that  some 
of  the  impurities  settle.  If  a  dry  gas  is 
needed,  the  drying  agent  used  depends  upon 
the  nature  of  the  gas.  Sulphuric  acid, 
calcium  chloride,  calcium  oxide,  potassium 
hydroxide,  etc.,  are  commonly  used,  and  the 
gas  finally  dried  if  necessary  by  phosphoric 
anhydride  mixed  with  beads  or  by  sodium. 
As  the  sodium  must  present  a  large  surface, 
it  may  be  used  as  wire  or  as  the  powder 


xii  GENERAL  DIRECTIONS 

obtained  when  it  is  melted  under  toluene  and 
shaken  violently  (care).  In  generating  a 
gas  a  safety  tube  should  always  be  used 
when  possible.  When  a  gas  is  being 
absorbed  by  a  liquid  precautions  should 
always  be  taken  to  prevent  the  liquid  run- 
ning back  into  the  generating  flask.  For 
this  purpose  the  delivery  tube  may  dip 
under  mercury,  the  wash-bottle  may  be  pro- 
vided with  a  valve,  etc.  An  excellent  device 
is  to  place  between  the  wash-bottle  and  the 
absorption  flask  an  empty  reversed  wash- 
bottle  large  enough  to  hold  all  the  absorb- 
ing liquid.  The  long  tube  of  the  wash- 
bottle  is  next  to  the  absorption  flask,  so 
that  if  liquid  runs  back  it  remains  in  the 
safety  bottle  as  long  as  all  the  gas  is 
absorbed,  and  any  gas  not  absorbed  forces 
it  back  into  the  absorption  flask. 

If  a  solid   is  formed  by  the  action  of  a 
gas  on    a   liquid,  the  delivery  tube  should 


GENERAL  DIRECTIONS  xiii 

have  a  wide  exit,  and  should  dip  just  below 
the  surface.  A  funnel  tube  is  well  adapted 
to  this  purpose. 

Always  absorb  excess  of  chlorine,  ammo- 
nia, sulphur  dioxide,  etc. 

The  gases  generally  used  in  the  labora- 
tory are  hydrogen,  oxygen,  nitrogen,  carbon 
dioxide,  hydrochloric  acid,  chlorine,  sulphur 
dioxide,  and  ammonia. 

Hydrogen  and  carbon  dioxide  generators 
must  always  be  on  hand.  Oxygen  and 
nitrogen  are  most  conveniently  used  from 
gasometers.  Nitrogen  may  be  made  by 
heating  gently  a  solution  of  60  grammes 
each  sodium  nitrite,  ammonium  chloride, 
and  potassium  bichromate  in  2  litres  water. 
It  is  purified  by  passing  over  hot  copper. 

The  most  convenient  source  of  gaseous 
hydrochloric  acid  is  the  concentrated  solu- 
tion. Some  of  this  is  placed  in  a  flask  with 
about  one-sixth  its  weight  of  common  salt 


xiv  GENERAL  DIRECTIONS 

and  concentrated  sulphuric  acid  slowly  added 
from  a  drop  funnel.  In  a  short  time  the  gas 
is  evolved,  and  may  be  controlled  by  regulat- 
ing the  flow  of  sulphuric  acid.  The  drop 
funnel  must  have  a  long  stem,  and  this  must 
be  full  of  sulphuric  acid  so  as  to  overcome 
the  pressure  of  the  liquid  in  the  wash-bottles. 

A  steady  stream  of  chlorine  may  be 
obtained  by  heating  in  a  water-bath  one 
part  pyrolusite  and  four  parts  crude  hydro- 
chloric acid  contained  in  a  flask  or  stone 
jug.  The  spent  liquid  should  not  be  thrown 
away  but  worked  for  manganous  chloride. 

Sulphur  dioxide  is  easily  obtained  by 
heating  on  asbestos  board  copper  turnings 
with  two  or  three  times  their  weight  of 
concentrated  sulphuric  acid.  The  addition 
of  a  few  small  pieces  of  charcoal  is  advis- 
able. Unless  entirely  used  up  the  acid 
should  be  separated  from  the  powder  that 
settles  to  the  bottom  and  kept  for  future 


GENERAL  DIRECTIONS  xv 

use.  The  powder  dissolved  in  water  yields 
crystals  of  copper  sulphate. 

Gaseous  ammonia  is  evolved  when  ammo- 
nia water  is  gently  heated.  It  should  be 
dried  with  lime  and  potassium  or  sodium 
hydroxide. 

Liquids  are  usually  purified  by  redistilla- 
tion collecting  the  fraction  or  fractions  with 
constant  boiling-point.  It  may  at  times  be 
necessary  to  distil  under  diminished  press- 
ure. For  that  purpose  the  apparatus  of 
Briihl  will  be  found  convenient.  Never  put 
the  distilling  flask  above  the  level  of  the 
eyes,  and  when  distilling  under  diminished 
pressure  always  use  goggles.  . 

In  distilling  always  leave  an  opening  for 
the  escape  of  any  gas  formed  and  of  the  air 
in  the  apparatus.  The  opening  may  be 
protected  from  the  air  and  moisture  by  a 
mercury  valve,  a  drying  tube,  etc.  When 
a  liquid  cannot  be  distilled  without  decom- 


xvi  GENERAL  DIRECTIONS 

position  it  may  be  identified  by  its  color, 
density,  index  of  refraction,  etc. 

Solids  may  usually  be  purified  by  recrys- 
tallization.  If  the  substance  is  much  less 
soluble  in  the  cold  than  in  the  hot  solvent,  a 
hot  saturated  solution  is  first  made  and  then 
cooled  rapidly  with  constant  stirring.  After 
one  or  more  repetitions  the  product  is  pure, 
and  large  crystals  may  now  be  obtained  by 
dissolving  in  little  cold  solvent  and  allowing 
to  evaporate  slowly.  Water  is  the  usual 
inorganic  solvent,  but  sometimes  it  is  neces- 
sary to  extract  with  alcohol,  ether,  etc. 
Occasionally  the  impure  product  is  dissolved 
and  the  impurity  or  the  substance  desired 
thrown  out  by  adding  another  liquid,  in 
which  it  is  insoluble. 

Solids  are  sometimes  purified  by  sublima- 
tion, though  for  obvious  reasons  this  is  less 
convenient  and  less  used  than  the  distilla- 
tion of  liquids. 


'    GENERAL  DIRECTIONS  xvii 

Organic  matter  is  frequently  objection- 
able, and  as  corks  and  rubber  are  almost 
indispensable,  they  may  be  protected  by 
wrapping  thin  asbestos  paper  around  the 
stoppers  or  around  the  ends  of  the  glass 
tubes  connected  by  the  rubber. 

It  is  not  usually  necessary  to  use  chemi- 
cally pure  reagents  in  making  preparations. 
Common  sense  must  here  be  the  guide. 

Complete  notes  should  be  kept.  It  is 
particularly  important  to  record  yield  and 
purity  of  products. 


xviii  GENERAL  DIRECTIONS 


ABBREVIATIONS  OF  REFERENCES 

A.  Liebig's  Annalen. 

A.  ch.  Annales  de  Chimie. 

A.  ch.  p.  Annales  de  Chimie  et  de  Physique. 

Am.  J.  Sc.  American  Journal  of  Science  and  Arts. 

A.  Min.  Annales  des  Mines. 

B.  Berichte  der  deutschen  chemischen  Gesell- 

schaft. 

Bl.  Bulletin  de  la  Societ£  chimique  de  Paris. 

Ch.  C.  Chemisches  Centralblatt. 

Ch.  N.          Chemical  News. 

C.  r.  Comptes-rendus  des  Seances  de  1' Academic 

des  Sciences. 

D.  Dingler's  Polytechnisches  Journal. 

J.  Jahresbericht    iiber    die    Fortschritte    der 

Chemie. 

J.  pr.  Journal  fur  praktische  Chemie. 

P.  A.  Poggendorf's  Annalen. 

Ph.  C.  Pharmaceutische  Centralhalle. 

Rec.  Recueil  des  Travaux  chimiques  des  Pays-Bas. 

Scher.  Scherer's  Journal  der  Chemie. 

Soc.  Journal  of  the  Chemical  Society  of  London. 

Z.  Zeitschrift  fur  Chemie  und  Pharmacie. 

Z.  Anorg.  Zeitschrift  fur  anorganische  Chemie. 

Z.  phys.  Zeitschrift  fur  physikalische  Chemie. 


INORGANIC    CHEMICAL 
PREPARATIONS 

SODIUM   CHLORIDE 

Wittstein,  Buchner's  Repertorium  65,  361. 

Dissolve  150  grammes  common  salt  in 
500  c.c.  water;  filter,  and  to  the  hot  solution 
add  milk  of  lime  containing  2j4  grammes 
calcium  hydroxide,  then  a  slight  excess  of 
barium  chloride.  Allow  to  stand,  filter,  and 
add  a  solution  of  5  grammes  sodium  car- 
bonate ;  heat  to  boiling,  filter,  neutralize 
with  dilute  hydrochloric  acid,  and  evaporate 
to  150  c.c.  as  rapidly  as  possible.  Collect 
the  sodium  chloride  on  a  platinum  cone, 
wash  with  little  hot  water,  and  dry  by 


2       INORGANIC  CHEMICAL  PREPARATIONS 

heating  gently  in  a  platinum  or  porcelain 
dish. 


POTASSIUM   CHLORATE 

Liebig,  A.  41,  307. 

Slake  75  grammes  quicklime,  mix  it 
with  30  grammes  potassium  chloride,  and 
add  sufficient  water  to  make  a  thin  paste. 
Heat  almost  to  boiling,  and  pass  in  chlorine 
(using  wide  delivery  tube)  until  no  more  is 
absorbed  and  all  the  lime  has  passed  into 
solution.  When  necessary  add  water  to 
keep  the  volume  constant.  Boil  for  one 
hour,  passing  carbon  dioxide  the  last  ten 
minutes,  and  filter  hot.  Evaporate  to 
100  c.c.,  and  set  aside  to  crystallize.  Evapo- 
rate the  mother  liquor  further,  and  again 
set  aside.  Purify  the  potassium  chlorate 
by  recrystallization  until  it  is  free  from 
chloride. 


BICARBONATE  OF  SODA  3 

BICARBONATE   OF   SODA 

Schlosing  &  Reliant,  A.  ch.  p.  (4)  14,  5. 
Mond,  Ch.  C.  1886,  189. 

Dissolve  100  grammes  salt  in  300  c.c. 
water,  and  saturate  the  solution  with 
ammonia,  keeping  it  cold  with  ice  water. 
Filter  if  necessary,  and  put  into  a  tall, 
narrow  cylinder.  Cork  the  cylinder,  and 
have  a  wide  glass  tube  pass  through  the 
cork,  and  dip  about  20  centimetres  below 
the  surface  of  the  liquid.  Connect  with  a 
carbon  dioxide  generator  (Kipp's),  uncork 
the  cylinder,  and  allow  carbon  dioxide  to 
pass  through.  When  all  the  air  is  expelled 
from  the  cylinder  cork  tightly,  and  allow 
carbon  dioxide  to  pass  in  as  rapidly  and  as 
long  as  it  will,  removing  the  cork  from 
time  to  time.  Filter  from  the  bicarbonate, 
wash  it  with  cold  water,  and  spread  it  out 
to  dry,  covering  it  with  filter  paper.  After 


4       INORGANIC  CHEMICAL  PREPARATIONS 

two    or    three    days   again   wash   with    ice 
water,  and  dry  at  40°. 

SODIUM   NITRITE 

Hampe,  A.  125,  336. 

Melt  85  grammes  sodium  nitrate  in  a 
small,  flat,  iron  dish  (sand-bath),  and  add 
slowly  206  grammes  granulated  lead.  Stir 
until  the  lead  is  completely  oxidized  (30-50 
minutes),  and  pour  the  molten  mass  upon 
an  iron  or  slate  slab.  Powder  and  wash 
thoroughly  with  boiling  water.  Cool  the 
filtrate,  pass  in  carbon  dioxide  for  a  few 
minutes,  heat  to  boiling,  and  filter  hot. 
Evaporate  until  crystals  separate  on  cooling. 
Unless  the  evaporation  has  been  carried 
too  far,  the  crystals  are  almost  pure  sodium 
nitrate.  Pour  off  the  solution,  again  evapo- 
rate and  cool,  and  repeat  until  the  solid 
shows  a  decided  test  for  nitrite.  Then 


BASIC  LEAD  NITRITE  5 

evaporate  the  mother  liquor  to  dryness,  and 
extract  repeatedly  with  boiling  absolute 
alcohol.  Evaporate  the  alcohol  and  recrys- 
tallize  from  water.  To  determine  the 
strength  of  the  nitrite,  dissolve  a  weighed 
portion  in  considerable  water,  add  the  quan- 
tity of  potassium  permanganate  it  would 
require  if  pure,  acidify  with  sulphuric  acid, 
and  titrate  the  excess  of  permanganate. 

BASIC   LEAD    NITRITE 

Chevreul,  A.  ch.  83,  72. 

Pdigot,  A.  ch.  p.  (3)  2,  87. 

v.  Lorenz,  Wien.  Akad.  Ber.  (2)  84,  1133. 

Dissolve  25  grammes  lead  nitrate  in  2 
litres  water,  add  gradually  50  grammes 
finely  granulated  lead,  and  heat  on  the 
water-bath  for  several  days.  Cool  in  ice 
water,  pass  in  carbon  dioxide  fifteen  min- 
utes, boil  two  or  three  minutes,  filter  hot, 
and  evaporate  to  crystallization. 


6       INORGANIC  CHEMICAL  PREPARATION'S 

CUPROUS   CHLORIDE 

Proust,  Scher.  8,  49. 
A.  ch.  28,  218;  32,  48. 

Dissolve  20  grammes  cupric  oxide  in 
200  c.c.  commercial  hydrochloric  acid  and 
heat  with  25  grammes  copper  turnings  until 
the  green  color  disappears.  Pour  the  liquid 
into  a  tall  cylinder  containing  at  least  i  litre 
distilled  water.  Allow  the  white  precipitate 
to  settle,  and  wash  it  with  very  dilute  hydro- 
chloric acid  until  the  washings  are  colorless, 
decanting  or  siphoning  off  the  liquid.  Then 
bring  the  precipitate  upon  a  filter,  and,  using 
a  filter-pump,  wash  as  rapidly  as  possible, 
first  with  very  dilute  hydrochloric  acid,  then 
with  alcohol,  and  finally  with  ether.  Until 
all  the  water  is  washed  out,  the  precipitate 
should  be  kept  covered  with  liquid  so  as  to 
protect  it  from  the  air.  If  the  precipitate 
is  white  after  washing,  bring  it  into  a  vacuum 


LEAD  DIOXIDE  7 

desiccator  over  paraffine  and  sulphuric  acid, 
and  when  dry  keep  in  a  tightly  stoppered 
bottle.  If  the  product  is  reddish  or  green, 
dissolve  it  in  concentrated  hydrochloric  acid, 
pour  into  water,  and  wash  as  before. 

LEAD   DIOXIDE 
Dry  Method 

Kassner,  D.  274,  136,  183,  226,  270. 
Archiv  der  Pharmacie,  228,  109. 

Mix  intimately  50  grammes  each  lead 
oxide  and  calcium  carbonate,  put  into  a  clay 
roasting  dish,  and  heat  for  thirty  minutes  to 
redness,  stirring  with  a  pipe-stem  so  as  to 
expose  the  hot  mass  to  the  action  of  the  air. 
Cool,  powder,  and  again  heat  for  thirty 
minutes,  repeating  the  operation  until  the 
color  no  longer  changes  on  heating.  Add 
the  powder  gradually  to  500  c.c.  dilute 
nitric  acid,  decant,  wash  two  or  three  times 


8       INORGANIC  CHEMICAL  PREPARATIONS 

with  200  c.c.  dilute  nitric  acid,  then  with  hot 
water,  and  dry  at  125°. 

Wet  Method 

Wohler,  A.  90,  383. 

Rivot,  Bendant  and  Dagum,  A.  Min.  (5)  4,  221. 

Bottger,  J.  pr.  76,  235. 

Dissolve  50  grammes  lead  acetate  in 
200  c.c.  water,  add  200  c.c.  sodium  hydroxide 
solution  (20%),  and  pass  in  chlorine  as  long 
as  any  action  is  observed.  Decant,  wash 
with  water,  boil  with  300  c.c.  dilute  nitric 
acid,  again  wash  with  water,  and  dry  at 
125°. 

MERCURIC   OXIDE 
Red  Mercuric  Oxide,  Dry  Method 

Heat  cautiously  10  grammes  mercuric 
nitrate  in  a  porcelain  crucible  until  red 
fumes  cease  to  come  off,  and  mercury  con- 
denses on  a  cold  crucible  cover  held  above 
the  heated  mass. 


BORIC  ACID  9 

Red  Mercuric  Oxide,  Wet  Method 
Bosetti,  Pharmaceut.  Zeitung  35,  471. 

To  a  boiling  solution  of  30  grammes 
mercuric  chloride  in  100  grammes  water 
add  a  hot  solution  of  barium  hydroxide  i  :  4, 
at  first  rapidly,  then  drop  by  drop,  until  the 
dark  brown  precipitate  changes  to  deep  red. 
Then  pour  into  4  litres  hot  water,  wash, 

and  dry. 

Yellow  Mercuric  Oxide 

Siewert,  A.  125,  226. 
Oswald,  Z.  phys.  18,  159. 
Bosetti,  loc.  cit. 

Dissolve  30  grammes  mercuric  chloride 
in  300  c.c.  water,  and  pour  the  solution  into 
250  c.c.  potassium  hydroxide  solution  (10%). 
Wash  and  dry. 

BORIC   ACID 

Dissolve  50  grammes  borax  in  200  c.c. 
boiling  water,  and  add  30  c.c.  concentrated 


10     INORGANIC  CHEMICAL  PREPARATIONS 

hydrochloric  acid.  Allow  to  stand  24  hours, 
and  collect  the  boric  acid  on  a  filter.  Wash 
it  with  little  cold  water,  and  heat  to  150° 
for  one  hour ;  dissolve  in  little  boiling  water 
and  allow  to  crystallize. 

BORON 

Jones,  Soc.  35,  41. 
Gattermann,  B.  22,  195. 
Winkler,  B.  23,  772. 
Moissan,  C.  r.  114,  392. 

Melt  250  grammes  borax  in  a  Hessian, 
crucible,  and  when  it  reaches  a  state  of 
quiet  fusion  pour  upon  a  slab.  Powder 
while  hot,  and  mix  at  once  25  grammes  with 
12  grammes  powdered  magnesium.  Put 
the  mixture  into  the  same  crucible,  pack 
tightly,  and  add  a  layer  of  the  fused  and 
powdered  borax.  Close  the  crucible  with 
a  well-fitting  cover.  (Work  as  rapidly  as 
possible.)  Heat  for  fifteen  to  twenty  min- 


SODIUM  THIOSULPHATE  II 

utes  to  redness.  When  the  crucible  is  cold 
break  it  and  remove  the  contents,  discard- 
ing carefully  adhering  pieces  of  crucible. 
Powder  and  boil  successively  with  water, 
concentrated  hydrochloric  acid  and  water. 
The  residue  is  impure  boron.  To  purify, 
mix  with  20  grammes  fused  borax  in  a 
Hessian  crucible,  add  a  layer  of  borax,  cover 
the  crucible,  and  put  it  in  a  bed  of  titanium 
oxide  and  charcoal  in  a  larger  crucible, 
surrounding  it  completely  with  the  mixture. 
Heat  and  wash  as  before,  repeating  if 
necessary. 

SODIUM   THIOSULPHATE 

Walchner,  A.  46,  235. 

Divide  into  two  equal  portions  a  hot 
saturated  aqueous  solution  of  200  grammes 
sodium  carbonate.  Keep  one  portion  warm 
on  the  water-bath,  pass  through  sulphi 


12     INORGANIC  CHEMICAL  PREPARATIONS 

dioxide  as  long  as  it  is  absorbed,  and  add 
at  once  the  other  portion.  Boil  the  solution 
of  sodium  sulphite  with  flowers  of  sulphur 
until  no  more  dissolves.  Filter,  evaporate 
to  a  small  bulk,  and  allow  to  crystallize. 
Purify  by  recrystallization. 

BARIUM   DITHIONATE 

Gay-Lussac  &  Welter,  A.  ch.  p.  10,  313. 
Spring  &  Bourgeois,  Bl.  (2)  46,  151. 

Suspend  50  grammes  precipitated  man- 
ganese dioxide  in  water,  put  the  flask  in  ice 
water,  and  lead  in  sulphur  dioxide  as  long 
as  anything  goes  into  solution.  Filter,  heat 
to  boiling,  cool,  and  add  barium  hydroxide 
solution  until  ammonium  sulphide  added  to 
a  small  portion  no  longer  gives  a  flesh- 
colored  precipitate.  Filter,  wash  the  pre- 
cipitate with  boiling  water,  add  the  washings 
to  the  main  filtrate,  heat  to  boiling,  and 
pass  in  carbon  dioxide  until  the  liquid  is 


SODIUM  AMMONIUM  PHOSPHATE          13 

neutral  to  litmus.     Filter  hot,  evaporate,  and 
allow  to  crystallize. 

AMMONIUM   NITRATE 

To  250  c.c.  nitric  acid  kept  cold  by  a 
freezing  mixture,  add  slowly  and  with  con- 
stant stirring  concentrated  ammonia  water 
in  slight  excess.  Allow  to  stand  over  night, 
and  separate  by  decantation  and  filtration 
from  any  brown  sediment.  Should  crystals 
separate,  redissolve  in  little  cold  water  and 
add  to  the  main  liquid.  Evaporate  on  the 
water-bath  until  the  density  of  the  hot  liquid 
is  1.25.  Allow  to  crystallize,  separate  the 
crystals,  dry  them  between  filter  paper,  and 
work  the  mother  liquor  further. 

SODIUM  AMMONIUM  PHOSPHATE 

Mitscherlich,  A.  ch.  p.  19,  399. 

Dissolve  375  grammes  crystallized  sodium 
phosphate  in  125  c.c.  water,  and  to  the  hot 


14     INORGANIC  CHEMICAL  PREPARATIONS 

solution  add  slowly  65  grammes  ammonium 
chloride.  When  all  is  dissolved  boil  for 
a  moment  and  filter,  using  hot  water  funnel. 
Cool  rapidly  with  constant  stirring  and 
drain  the  crystals.  Redissolve  in  75  c.c. 
boiling  water  and  recrystallize  adding  a  little 
ammonia.  Repeat  until  free  from  sodium 
chloride.  Dry  at  30°  and  keep  in  well- 
closed  bottle. 

ZINC  —  FREE   FROM    ARSENIC 
L'Hote,  C.  r.  98,  1491. 

Melt  500  grammes  zinc  in  a  Hessian 
crucible,  and  by  means  of  a  thick  iron  wire 
hold  6  to  8  grammes  magnesium  chloride 
below  the  surface  of  the  molten  mass,  stirring 
gently.  When  all  the  magnesium  chloride 
has  disappeared,  heat  almost  to  the  boiling- 
point  of  zinc  15  minutes,  then  allow  the  zinc 
to  cool  somewhat  and  granulate  by  pouring 
into  water. 


CHROME  ALUM  15 

ARSENIC  ACID 

Kopp,  C.  r.  42,  1060. 

In  a  retort  heat  100  grammes  arsenious 
oxide  in  small  pieces  (why  not  in  powder  ?) 
with  100  c.c.  fuming  nitric  acid.  When 
fumes  are  no  longer  evolved,  pour  off  the 
liquid  and  evaporate  to  dryness.  Test  for 
arsenious  acid,  and  if  any  is  present  add 
aqua  regia  and  again  evaporate  to  dryness. 
Again  test  for  arsenious  acid  and  repeat 
evaporation  with  aqua  regia  until  free  from 
arsenious  acid.  Then  dissolve  in  boiling 
water  and  evaporate  to  a  thin  syrup.  Heat 
on  the  water-bath  until  crystals  form  on 
cooling. 

CHROME    ALUM 

Bottger,  J.  pr.  36,  318. 
Traube,  A.  66,  169. 

Dissolve  ioo  grammes  potassium  bichro- 
mate in  400  c.c.  warm  water,  add  140 


16     INORGANIC  CHEMICAL  PREPARATIONS 

grammes  sulphuric  acid  and  cool  to  30°. 
Add  slowly  alcohol  until  there  is  no  further 
action,  taking  care  to  keep  the  temperature 
below  50°.  Cool  to  zero  and  decant  from 
the  crystals.  Evaporate  the  liquid  to  icoc.c., 
keeping  the  temperature  below  50° ;  again 
cool  to  zero  and  decant  from  the  crystals. 
Combine  the  two  crops  and  purify  by  re- 
crystallization,  keeping  the  temperature  of 
the  solution  below  50°. 

CHROMIC  ANHYDRIDE 

Bolley,  A.  56,  113. 
Traube,  A.  66,  169. 

Dissolve  300  grammes  potassium  bichro- 
mate in  500  c.c.  water,  add  420  c.c.  sulphuric 
acid,  and  allow  to  stand  over  night.  Filter 
through  glass  wool  and  wash  the  acid  potas- 
sium sulphate  with  not  over  10  c.c.  cold 
water.  To  the  filtrate  add  20  c.c.  sulphuric 


CHROMOUS  ACETATE  17 

acid  and  evaporate  until  chromic  acid  begins 
to  separate.  Allow  to  stand  over  night  and 
collect  on  a  platinum  cone.  Wash  with 
50  c.c.  nitric  acid  and  dry  in  desiccator 
over  potassium  hydroxide. 

CHROMOUS   ACETATE 

Moissan,  A.  ch.  p.  (5)  25,  416. 

Heat  50  grammes  chromic  anhydride  with 
500  c.c.  fuming  hydrochloric  acid  until  no 
more  chlorine  is  evolved.  Evaporate  to 
200  c.c.,  pour  the  liquid  upon  250  grammes 
granulated  zinc  in  a  large  flask,  and  add 
125  c.c.  hydrochloric  acid.  When  the  first 
violent  action  is  over,  place  in  the  neck  of 
the  flask  a  rubber  stopper  carrying  two 
tubes,  one  terminating  just  below  the  stop- 
per, the  other  going  to  the  bottom  of  the 
flask.  Connect  the  longer  with  a  bent  tube 
reaching  below  the  surface  of  a  solution  of 
400  grammes  crystallized  sodium  acetate 


1 8     INORGANIC  CHEMICAL  PREPARATIONS 

in  ij  litres  water.  When  the  liquid  is  a 
pure  blue,  close  the  shorter  tube  and  the 
hydrogen  evolved  will  force  the  liquid  into 
the  sodium  acetate  solution.  If  necessary 
filter  the  chromous  chloride  solution  by 
inserting  a  bulb  tube  with  glass  wool.  Wash 
the  red  precipitate  of  chromous  acetate 
repeatedly  with  boiled  water  through  which 
carbon  dioxide  has  been  passed,  and  keep 
as  a  paste.  Keep  the  flask  containing  the 
chromous  acetate  full  of  carbon  dioxide 
while  washing,  and  siphon  off  the  water  used 
for  washing. 

HYDROBROMIC   ACID 

Linnemann,  A.  161,  198. 

Mix  10  grammes  red  phosphorus  with 
80  grammes  sand,  put  into  a  small  flask  and 
moisten  with  20  grammes  water.  Close  the 
flask  with  a  stopper  carrying  a  glass  tube 


H  YD  RIO  TIC  ACID  19 

and  a  drop  funnel,  and  by  means  of  the 
latter  gradually  drop  in  60  grammes  bromine. 
Pass  the  gaseous  hydrobromic  acid  through 
a  U-tube  containing  moist  red  phosphorus 
mixed  with  plenty  of  beads  or  pieces  of 
glass  and  then  into  60  grammes  water.  To 
prevent  water  running  back,  pass  the  delivery 
tube  into  the  tubular  of  a  small  retort  whose 
neck  dips  into  the  60  grammes  water  con- 
tained in  a  beaker.  Loss  of  bromine  may 
be  avoided  and  a  steady  flow  obtained  by 
closing  the  drop  funnel  with  a  cork  through 
which  a  glass  tube  drawn  to  a  capillary  is 
passed.  Determine  the  strength  of  the 
aqueous  acid  obtained. 

HYDRIODIC   ACID 

Naumann,  A.  151,  145. 
Berthelot,  C.  r.  76,  741. 

Powder   50  grammes   iodine,  suspend   it 
in  250  c.c.  water  in  a  500  c.c.  flask  and  pass 


20     INORGANIC  CHEMICAL  PREPARATIONS 

in  hydrogen  sulphide.  Provide  the  flask 
containing  the  iodine  and  water  with  a 
stopper  through  which  the  delivery  tube 
passes,  and  as  soon  as  all  the  air  is  displaced, 
close  the  flask  and  leave  it  connected  with 
the  hydrogen  sulphide  generator  over  night. 
If  the  iodine  has  not  all  disappeared,  lift 
the  stopper  every  hour  for  a  minute  or  two 
and  shake  vigorously  from  time  to  time.  As 
soon  as  the  iodine  has  disappeared,  heat 
gently  on  water-bath  passing  hydrogen 
through  to  drive  out  excess  of  hydrogen 
sulphide.  Filter  from  sulphur,  and  distil 
in  a  current  of  hydrogen,  collecting  the  por- 
tion between  125°  and  130°.  Sometimes 
the  iodine  gets  coated  with  sulphur  and  is 
not  further  acted  upon.  It  must  then  be 
removed  and  powdered.  If  large  quantities 
of  hydriodic  acid  are  to  be  made,  it  is  advisa- 
ble to  dissolve  the  iodine  instead  of  suspend- 
ing it 


TIN  TETRACHLORIDE  21 

Fifty  to  sixty  grammes  hydriodic  acid 
may  be  made  as  above  and  without  first 
concentrating  used  to  dissolve  the  iodine. 


TIN   TETRACHLORIDE 

Lorenz,  Z.  Anorg.  10,  44. 

Seal  one  end  of  a  glass  tube  2  or  3  centi- 
metres in  diameter  and  40  centimetres  long 
and  fit  into  it  a  double  bored  rubber  stopper. 
Through  one  of  the  holes  pass  an  inverted 
condenser,  and  through  the  other  a  long 
glass  tube  that  may  be  raised  or  lowered. 
Fill  the  larger  tube  with  granulated  tin, 
have  the  delivery  tube  reach  to  the  bottom 
and  pass  in  dry  chlorine.  Liquid  tin  tetra- 
chloride  soon  forms.  Move  the  delivery 
tube  so  that  it  just  dips  into  the  liquid,  and 
pass  the  chlorine  until  action  ceases.  Pour 
from  the  little  tin  usually  left,  purify  by 


22     INORGANIC  CHEMICAL  PREPARATIONS 

redistillation  and  keep  in  sealed  tubes.     Tin 
tetrachloride  boils  at  114°. 


SULPHURYL   CHLORIDE 

Schulze,  J.  pr.  (2)  24,  168. 

Put  30  grammes  camphor  into  an  absorp- 
tion flask,  place  in  ice  water  and  lead  in 
sulphur  dioxide  as  long  as  it  is  absorbed. 
Then  lead  in  chlorine  until  it  passes  through 
unabsorbed,  then  sulphur  dioxide  and  chlo- 
rine in  rotation  until  the  liquid  no  longer 
increases  in  bulk.  Put  into  a  retort  and 
collect  the  portion  coming  over  below  100°. 
If  required,  the  portion  boiling  above  100° 
may  be  treated  in  the  same  way  as  the 
camphor,  i.e.  sulphur  dioxide  and  chlorine 
led  in  alternately,  and  thus  a  large  quantity 
of  low  boiling  liquid  obtained  from  little 
camphor.  The  low  boiling  liquid  is  sub- 


PHOSPHORUS  TRICHLORIDE  23 

jected  to  fractional  distillation,  the  sulphuryl 

chloride  coming  over  between  68°  and  71°. 

-», 

PHOSPHORUS   TRICHLORIDE 

Michaelis,  Graham-Otto's  Lehrbuch  II.  324. 

Cover  the  bottom  of  a  tubulated  retort 
with  dry  sand  and  connect  with  a  double- 
necked  receiver,  protecting  the  corks  with 
asbestos  paper.  In  the  second  neck  of  the 
receiver  put  a  drying  tube  and  absorb  the 
gas  which  passes  this  in  sodium  hydroxide 
solution,  using  a  safety  bottle  or  mercury 
valve.  (If  no  double-necked  receiver  is  at 
hand,  an  ordinary  flask  and  double-bored 
cork  may  be  used.)  Fill  the  apparatus  with 
carbon  dioxide,  throw  in  100  grammes  yellow 
phosphorus  dried  between  filter  paper,  and 
then  dipped  successively  into  alcohol  and 
ether,  again  pass  carbon  dioxide  for  fifteen 
minutes,  put  the  retort  into  a  pail  of  warm 


24    INORGANIC  CHEMICAL  PREPARATIONS 

water  and  pass  in  a  current  of  chlorine. 
The  chlorine  delivery  tube  must  move  easily 
in  the  stopper  so  that  it  may  be  raised  or 
lowered.  If  the  end  of  the  tube  is  too 
near  the  phosphorus,  the  latter  gets  hot  and 
distils,  forming  a  red  crust.  If  the  tube 
is  too  far  away,  the  action  is  slow,  the  excess 
of  chlorine  acts  and  phosphorus  pentachlo- 
ride  is  formed.  The  position  must  be  such 
that  the  retort  remains  uncoated.  As  soon 
as  action  begins,  as  indicated  by  a  tongue 
of  flame  from  the  tube  to  the  phosphorus, 
the  retort  may  be  removed  from  the  hot 
water,  but  water  should  always  be  kept 
under  the  retort  to  catch  the  phosphorus 
in  case  of  accident.  Toward  the  end,  the 
voluminous  phosphorus  remaining  may  be 
cautiously  heated.  Purify  the  trichloride 
by  redistillation,  excluding  water.  Be  care- 
ful not  to  inhale  any.  Boiling-point  74°. 


ANTIMONY  TRICHLORIDE  2$ 

FLUORSILICIC   ACID 

Berzelius,  J.  1825,  89;  P.  A.  I,  169. 
Stolba,  D.  197,  336. 

Mix  50  grammes  each  fluor-spar  and  sand, 
and  heat  in  an  old  flask  with  150  c.c.  sul- 
phuric acid.  Lead  the  gas  evolved  through 
an  empty  flask,  and  then  into  200  c.c.  water, 
using  a  mercury  valve  or  a  thistle  tube. 
When  the  action  is  over  press  the  liquid 
from  the  separated  silicic  acid,  wash  with 
little  water,  and  filter.  Determine  strength 
of  acid  by  titration. 

ANTIMONY   TRICHLORIDE 

In  a  500  c.c.  flask  heat  50  grammes  gray 
antimony  ore  with  250  c.c.  concentrated 
hydrochloric  acid,  adding  gradually  a  few 
grammes  potassium  chlorate.  As  soon  as 
all  the  ore  is  acted  upon  filter  through 


26     INORGANIC  CHEMICAL  PREPARATIONS 

glass  wool  and  evaporate  to  100  c.c.  Pour 
into  2000  c.c.  water,  wash  the  precipitate 
with  cold  water,  and  dissolve  it  in  75  c.c. 
concentrated  hydrochloric  acid,  leading  in 
gaseous  hydrochloric  acid  until  no  more  is 
absorbed.  Pour  the  solution  into  a  tubu- 
lated retort  containing  some  bits  of  glass  to 
prevent  bumping,  and  distil.  As  soon  as  a 
drop  of  the  distillate  gives  a  white  precipi- 
tate with  water  change  the  receiver,  and  do 
this  again  when  the  distillate  begins  to 
solidify  on  a  glass  rod.  The  last  portion 
is  antimony  trichloride,  a  white  crystalline 
substance.  If  colored  by  iron  it  must  be 
redissolved  in  concentrated  hydrochloric 
acid  and  redistilled.  The  portion  of  the 
distillate  that  gives  a  white  precipitate  with 
water  is  a  solution  of  antimony  trichloride 
in  hydrochloric  acid,  and  may  be  used  for 
the  next  preparation. 


SILVER  NITRATE  2J 

ANTIMONY   OXYCHLORIDE 

Johnston,  J.  pr.  6,  55. 
Malaguti,  A.  ch.  p.  59,  220. 
P£ligot,  A.  ch.  p.  (3)  20,  288. 

Powder  of  Algaroth 

Pour  the  acid  solution  of  antimony  tri- 
chloride obtained  in  the  previous  experiment 
into  400-500  c.c.  water,  wash  the  precipitate 
carefully,  dry  and  preserve. 

SILVER   NITRATE 

Place  a  porcelain  crucible  in  a  Hessian 
crucible  with  a  layer  of  sand  between  them. 
Cover  the  sand  with  fused  borax,  and  heat 
to  redness.  Gradually  bring  into  the  hot 
porcelain  crucible  a  mixture  of  100  grammes 
silver  chloride,  100  grammes  dry  sodium 
carbonate,  and  15  grammes  potassium 
nitrate.  Add  slowly,  or  it  may  foam  over. 


28     INORGANIC  CHEMICAL  PREPARATIONS 

When  the  mass  is  in  quiet  fusion  stir  with  a 
pipe-stem,  allow  to  settle,  cool  slightly,  and 
pour  the  contents  of  the  porcelain  crucible 
into  water.  The  coating  of  borax  should 
keep  sand  from  dropping  in.  Brush  the 
silver  clean,  and  boil  for  a  few  minutes  with 
dilute  sulphuric  acid.  Wash,  dissolve  in 
nitric  acid,  evaporate  to  dry  ness,  and  recrys- 
tallize  from  water.  . 

From  the  silver  residues  of  the  laboratory 
(chloride,  bromide,  cyanide,  etc.),  the  chlo- 
ride may  be  obtained  as  follows :  Dissolve 
the  residues  in  10%  potassium  cyanide  solu- 
tion, and  digest  on  the  water-bath  with  zinc 
dust  until  all  silver  is  precipitated.  Wash 
with  water,  boil  with  hydrochloric  acid, 
again  wash  thoroughly  with  water,  dissolve 
in  nitric  acid,  and  precipitate  with  hydro- 
chloric acid.  If  necessary,  redissolve  in 
ammonia,  and  precipitate  with  hydrochloric 
acid. 


SILVER  HYPONITRITE  29 

SILVER    HYPONITRITE 

Divers,  Ch.  N.  23,  206. 
Divers  &  Haga,  Soc.  45,  78. 
Van  der  Plaats,  B.  10,  1507. 
Miihlhauser,  Z.  1864,  720. 

Dissolve  10  grammes  sodium  nitrite  in 
30  grammes  water,  cool  in  ice  water,  and  add 
slowly  250  grammes  3%  sodium  amalgam. 
When  action  ceases  pour  from  the  mercury, 
neutralize  with  acetic  acid,  and  precipitate 
with  silver  nitrate.  To  get  rid  of  any  silver 
acetate  in  the  precipitate  expose  to  diffused 
sunlight  for  a  few  hours,  dissolve  in  very 
dilute  sulphuric  acid,  and  precipitate  with 
ammonia,  carefully  avoiding  an  excess. 
Wash  with  a  little  ice  water,  and  dry  in 
desiccator.  Keep  all  solutions  ice  cold,  and 
avoid  direct  sunlight. 

To  prepare  sodium  amalgam,  heat  sodium 
to  90°  under  low  melting  paraffine,  and  pour 


30    INORGANIC  CHEMICAL  PREPARATIONS 

in  the  mercury  in  a  fine  stream,  stirring  con- 
stantly. The  operation  is  harmless,  but 
should  be  carried  on  in  the  hood.  When 
working  with  molten  sodium  use  care,  and 
protect  the  eyes  with  goggles. 

STRONTIUM   CHLORIDE^ 

Berthier,  A.  ch.  p.  22,  231. 

In  a  Hessian  crucible  heat  to  bright  red- 
ness for  two  hours  a  mixture  of  200  grammes 
celestine  and  75  grammes  charcoal.  When 
cool  powder,  and  add  to  2  litres  dilute  hydro- 
chloric acid  5  %.  Heat  to  boiling,  filter  hot, 
and  evaporate  to  dryness.  Redissolve  in 
water,  remove  iron,  etc.  by  ammonium  sul- 
phide, and  barium  by  digesting  with  stron- 
tium sulphate,  and  recrystallize. 

STRONTIUM    HYDROXIDE 

Dissolve  75  grammes  strontium  chloride 
in  boiling  water,  add  75  grammes  sodium 


MANGANESE  31 

hydroxide  solution  (30  %),  cool,  collect  on  a 
platinum  cone,  and  wash  with  cold  water. 

MANGANOUS   CHLORIDE 

Everitt,  Phil.  Mag.  6,  193. 
Kolbe,  J.  pr.  (2)  5,  445. 

Evaporate  to  dryness  i  litre  of  the  liquid 
obtained  in  making  chlorine  from  manga- 
nese dioxide  and  hydrochloric  acid.  Heat 
the  residue  for  several  hours,  cool,  wash 
with  boiling  water,  and  filter.  To  ^  of  the 
filtrate  add  sodium  carbonate,  wash  the  pre- 
cipitate, and  digest  it  on  the  water-bath  with 
the  main  portion  until  ammonium  sulphide 
gives  a  ffesh-colored  precipitate  entirely  sol- 
uble in  dilute  acetic  acid.  Filter  and  recrys- 
tallize. 

MANGANESE 

Glatzel,  B.  22,  2857. 

Heat  150  grammes  manganous  chloride 
until  anhydrous,  and  mix  75  grammes  of  the 


32     INORGANIC  CHEMICAL  PREPARATIONS 

anhydrous  salt  with  100  grammes  dry  potas- 
sium chloride  and  50  grammes  anhydrous 
calcium  chloride.  Pack  the  mixture  in  a 
Hessian  crucible,  and  heat  to  quiet  fusion. 
Then  add  18  grammes  magnesium  in  pieces 
of  3  to  4  grammes.  As  each  piece  is 
thrown  in  cover  the  crucible,  and  wait  until 
the  action  is  over  before  adding  another. 
If  the  mass  is  too  hot  it  will  foam  over. 
Therefore,  have  it  as  cold  as  is  consistent 
with  complete  fusion  while  adding  the  mag- 
nesium, but  as  soon  as  all  the  magnesium 
is  in  bring  to  a  white  heat  as  rapidly  as 
possible.  Keep  at  white  heat  20-30  min- 
utes. Allow  to  cool,  break  the  crucible, 
and  wash  the  regulus  of  manganese.  If  the 
mass  was  brought  to  a  white  heat  imme- 
diately on  adding  the  magnesium,  the  man- 
ganese will  be  in  one  or  two  pieces  at  or 
near  the  bottom.  Otherwise  it  will  be  found 
as  small,  fairly  stable  pellets,  or  as  an 


IODINE  TRICHLORIDE  33 

unstable    powder    distributed    through   the 
mass. 

IODINE   TRICHLORIDE 

Brenken,  B.  8,  487. 

Connect  a  large-necked  flask  or  double- 
necked  receiver  with  both  a  chlorine  genera- 
tor and  a  small  retort  holding  15  grammes 
iodine,  taking  care  to  leave  an  outlet  for  the 
air.  Fill  the  receiver  with  dry  chlorine,  and 
slowly  distil  the  iodine,  generating  chlorine 
in  the  meanwhile  as  fast  as  it  is  used  up  so 
as  to  always  have  an  excess  of  chlorine  in 
the  receiver.  When  all  the  iodine  has  been 
used  up,  drive  out  the  excess  of  chlorine  by 
passing  air  through  the  apparatus.  Remove 
the  crystals  from  the  walls,  and  keep  in 
sealed  tube.  The  portion  which  cannot  be 
loosened  may  be  dissolved  in  water  and  the 
solution  kept. 


34    INORGANIC  CHEMICAL  PREPARATIONS 

IODIC   ACID 

Kammerer,  J.  pr.  79,  94. 

Heat  gently  in  a  hard  glass  flask  15 
grammes  iodine  and  80  grammes  fuming 
nitric  acid,  passing  a  current  of  air  through 
the  liquid.  If  the  iodine  does  not  all  dis- 
solve, add  more  fuming  nitric  acid  from  time 
to  time  until  it  does.  Evaporate  to  a  small 
bulk,  and  recrystallize  from  rather  dilute  hot 
nitric  acid  until  the  product  is  white. 

POTASSIUM   FLUORTITANATE 

Wohler,  A.  ch.  p.  (3)  29,  185. 

Heat  to  redness  25  grammes  rutile,  and 
throw  into  cold  water.  Dry,  reduce  to  a 
fine  powder,  mix  with  50  grammes  potas- 
sium carbonate  and  fuse  in  a  platinum 
crucible  placed  inside  of  a  Hessian  crucible. 
Cool,  powder,  and  dissolve  in  hot  dilute 


SULPHUR  MONOBROMIDE  35 

hydrofluoric  acid,  avoiding  much  excess  of 
the  latter.  Evaporate  to  small  bulk  and 
allow  to  cool.  Decant,  wash  the  potassium 
fluortitanate  with  ice-cold  water,  and  purify 
by  recrystallization. 

TITANIC   OXIDE 

Wohler,  A.  ch.  p.  (3)  29,  186. 

To  the  cold  mother  liquor  obtained  in  pre- 
paring potassium  fluortitanate  add  ammonia 
in  slight  excess,  and  filter  at  once  from  the 
brown  precipitate.  Heat  to  boiling,  collect 
and  dry  the  white  precipitate. 

SULPHUR   MONOBROMIDE 

Muir,  Soc.  28,  845. 

Wash  and  dry  carefully  20  grammes 
flowers  of  sulphur,  and  add  it  gradually  to 
50  grammes  bromine,  shaking  thoroughly 
after  each  addition.  Distil  carefully,  heat- 
ing to  225°-23o°.  Purify  by  redistillation. 


36    INORGANIC   CHEMICAL  PREPARATIONS 

NITROGEN    IODIDE 

Mallet,  Ch.  N.  39,  257. 

Dissolve  2  grammes  iodine  in  20  grammes 
warm  alcohol,  and  pour  into  200  c.c.  cold 
water.  Wash  the  powder  carefully  with 
water,  put  it  into  a  beaker,  pour  upon  it 
50  c.c.  strong  ammonia  water  at  zero,  and 
decant.  Repeat  twice,  using  no  rod  or 
other  solid  to  stir.  Wash  with  alcohol  two 
or  three  times,  then  with  absolute  alcohol, 
and  finally  with  ether.  Divide  into  small 
portions  before  the  final  washing.  Care!!! 
The  nitrogen  iodide  cannot  be  kept. 

NITROGEN    TETROXIDE 

Gay-Lussac,  A.  ch.  p.  i,  405. 

Powder  and  dry  100  grammes  lead  nitrate. 
Heat  it  in  a  hard  glass  tube  or  retort  to  dull 
redness,  passing  the  fumes  into  an  empty 


NITRIC  ANHYDRIDE  37 

wash  bottle  kept  at  30°,  then  into  a  U-tube 
containing  fused  calcium  nitrate,  and  finally 
into  a  dry  U-tube  kept  in  ice  water  and  pro- 
tected from  the  moisture  of  the  air  by  a 
calcium  nitrate  tube.  Pass  dry  air  or  oxy- 
gen into  the  liquid  thus  obtained  until  it  is 
straw  colored.  Keep  in  sealed  tubes.  Care 
must  be  taken  to  protect  the  nitrous  fumes 
from  organic  matter;  therefore  corks  must 
be  wrapped  in  asbestos  paper.  Where  glass 
tubes  are  connected  by  rubber,  wrap  the 
glass  in  asbestos  paper  and  put  the  rubber 
over  it,  tying  with  string  if  necessary. 

NITRIC   ANHYDRIDE 

Weber,  J.  pr.  (2)  6,  342. 
Berthelot,  Bl.  (2)  21,  53. 

To  200  c.c.  concentrated  colorless  nitric 
acid  add  slowly  100  c.c.  sulphuric  acid,  keep- 
ing cold.  Distil  gently  until  1 50  c.c.  passes 


38     INORGANIC  CHEMICAL  PREPARATIONS 

over.  To  the  distillate  add  100  c.c.  sul- 
phuric acid,  and  again  distil,  collecting 
100  c.c.,  to  which  add  75  c.c.  sulphuric  acid, 
and  again  distil,  collecting  50  c.c.,  which 
must  be  carefully  protected  from  moisture 
and  organic  matter.  Put  the  distillate  into 
a  tubulated  retort,  and  add  30  grammes 
phosphoric  anhydride  mixed  with  beads, 
keeping  below  zero.  When  the  whole  is 
thoroughly  mixed  keep  at  zero  for  a  few 
minutes,  then  allow  it  to  come  gradually  to 
the  temperature  of  the  room,  and  finally 
heat  in  a  water-bath  until  nitric  anhydride 
comes  over.  Collect  in  a  small  flask  kept  in 
ice,  and  use  at  once.  If  the  distillation  is 
carried  too  far  a  liquid  collects  on  the 
crystals  of  nitric  anhydride.  It  should  be 
poured  off.  It  is  not  as  a  rule  necessary 
to  make  connection  between  the  retort  and 
receiver  tight  to  exclude  moisture.  Organic 
matter  must  be  rigidly  excluded  and  a  vent 


SULPHURIC  ANHYDRIDE  39 

provided  for  the  escape  of  gas.  Usually 
nitric  anhydride  comes  over  when  the  tem- 
perature of  the  water-bath  reaches  60°.  It 
must  not  get  above  70°,  and  should  be  kept 
as  near  60°  as  is  consistent  with  the  distilla- 
tion of  nitrogen  pentoxide. 


SULPHURIC   ANHYDRIDE 

Osann,  D.  151,  158. 
Weber,  P.  A.  159,  315. 

Into  a  retort  about  one-third  full  of  fum- 
ing sulphuric  acid  put  a  platinum  spiral  long 
enough  to  project  above  the  surface  of  the 
liquid  and  distil,  collecting  the  first  fourth. 
Redistil  and  keep  the  product  in  sealed 
tubes.  While  distilling  protect  from  mois- 
ture and  organic  matter.  Leave  a  vent  for 
the  escape  of  gas.  As  a  precaution  put  a 
porcelain  jar  under  the  retort. 


40     INORGANIC  CHEMICAL  PREPARATIONS 

ALUMINIUM   CHLORIDE 

Escales,  B.  30,  1314. 

Fit  a  tubulated  bell-jar  with  a  glass  plate, 
and  cover  the  glass  plate  within  the  jar 
with  asbestos  paper.  Put  upon  the  asbestos 
paper  an  evaporating  dish  containing  30 
grammes  aluminium  filings.  Pass  in  hydro- 
chloric acid,  and  as  soon  as  all  the  air  is 
expelled  heat  a  little  aluminium  to  redness, 
and  lifting  the  stopper  drop  it  upon  the 
aluminium  in  the  dish.  The  action  con- 
tinues without  further  heating  if  a  lively 
current  of  hydrochloric  acid  is  passed  in. 
Should  the  action  stop,  pass  in  hydrochloric 
acid  until  all  the  hydrogen  is  out,  and  drop 
in  more  aluminium  heated  to  redness. 
When  all  the  aluminium  is  used  up  re- 
move the  aluminium  chloride  from  the  sides 
and  bottom,  and  keep  in  tightly  closed 
bottles. 


POTASSIUM  PERMANGANATE  41 

POTASSIUM   PERMANGANATE 

Aschoff,  J.  pr.  81,  29. 
Bottger,  J.  pr.  90,  157. 
Graeger,  J.  pr.  96,  169. 

In  an  iron  dish  fuse  20  grammes  potas- 
sium hydroxide,  5  grammes  potassium  chlo- 
rate, and  5-6  c.c.  water.  Remove  the  flame, 
and  slowly  add  20  grammes  powdered  man- 
ganese dioxide,  stirring  constantly.  Heat  to 
dull  redness  until  the  mass  is  hard  and  dry. 
Repeat  three  or  four  times  with  new  por- 
tions, unite,  and  powder.  Boil  the  powder 
with  2  litres  water,  leading  carbon  dioxide 
and  air  into  the  boiling  solution  until  a  drop 
leaves  a  red  mark  on  paper.  Filter  through 
glass  wool  or  a  Pasteur-Chamberland  filter, 
wash  the  residue  thoroughly,  and  evaporate 
until  crystals  form  on  cooling.  Allow  to 
stand  twenty-four  hours,  pour  from  the  crys- 
tals, concentrate  the  mother  liquor,  and 


42     INORGANIC  CHEMICAL  PREPARATIONS 

again  allow  to  crystallize,  repeating  until 
the  crystals  are  plainly  not  permanganate. 
Redissolve  all  the  crystals  in  boiling  water, 
filter  through  a  Pasteur-Chamberland  filter, 
and  recrystallize,  excluding  all  organic  mat- 
ter. Or  redissolve  all  the  crystals  in  cold 
water,  let  stand  a  week,  decant  carefully 
from  the  mud,  filter  through  glass  wool, 
and  evaporate  to  crystallization,  excluding 
organic  matter. 

CRYSTALLIZED   SILICON 

Caron,  A.  ch.  p.  (3)  63,  26. 

Deville  &  Caron,  A.  ch.  p.  (3)  67,  437. 

Vigouroux,  A.  ch.  p.  (7)  12,  50. 

Mix  75  grammes  potassium  fluorsilicate, 
100  grammes  granulated  zinc,  and  20 
grammes  sodium  in  small  pieces.  Throw 
the  mixture  into  a  red-hot  crucible,  and 
cover  immediately.  Unless  the  contents  of 


SILICOCHLOROFORM  43 

the  crucible  become  liquid  at  once,  heat  to 
fusion  and  stir  with  a  pipe-stem  for  a  minute 
or  two.  Cool  slowly,  separate  the  lump  of 
zinc,  wash  it  carefully,  and  treat  with  com- 
mercial hydrochloric  acid.  Wash  the  resi- 
due, heat  with  concentrated  nitric  acid  for  a 
few  minutes,  wash  thoroughly,  heat  with 
hydrofluoric  acid,  wash  and  dry. 

SILICOCHLOROFORM 

Friedel  &  Ladenburg,  A.  143,  118. 
Gattermann,  B.  22,  186,  190. 
Gattermann  &  Weinlig,  B.  27,  1943. 
Vigouroux,  A.  ch.  p.  (7)  12,  31. 

Dry  25  grammes  magnesium  in  the  air- 
bath  at  150°,  and  while  still  warm  (60°  to 
70°)  mix  with  40  grammes  warm  sand  pre- 
viously heated  to  redness,  and  then  placed  in 
a  desiccator.  Put  the  mixture  into  a  small, 
flat,  iron  dish  (sand-bath),  pour  upon  it  a 


44     INORGANIC  CHEMICAL  PREPARATIONS 

coating  of  dry  magnesium  oxide,  and  cover 
with  an  iron  plate  or  asbestos  board.  Heat 
to  redness  in  one  place  with  a  Bunsen 
burner.  As  soon  as  action  begins  the  part 
heated  glows,  and  the  burner  may  be  re- 
moved as  the  action  continues  throughout 
the  whole  mass.  When  cold  throw  into 
cold  water,  and  add  hydrochloric  acid  care- 
fully (Hood).  Decant,  add  concentrated 
hydrochloric  acid,  and  boil  for  half  an  hour. 
Cool,  decant,  and  wash  with  hot  water  until 
free  from  magnesia  and  hydrochloric  acid. 
Put  the  impure  silicon  into  a  combustion 
tube,  and  heat  to  redness  in  a  current  of 
hydrogen.  Cool  to  dull  redness,  connect 
one  end  with  a  receiver  (U-tube  or  spiral) 
and  the  other  with  a  generator  of  gaseous 
hydrochloric  acid.  Put  the  receiver  into 
ice  and  brine.  To  its  free  end  attach  a 
drying  tube,  and  to  this  a  delivery  tube 
dipping  into  water.  Pass  a  steady  stream  of 


HYDROGEN  PERSULPHIDE  45 

the  carefully  dried  hydrochloric  acid,  keep- 
ing the  combustion  tube  at  or  just  below 
dull  red  heat  The  water  is  soon  covered 
with  flaky  silico-formic  anhydride,  and  unless 
the  delivery  tube  is  dry  and  wide  it  soon 
gets  stopped  up.  A  mixture  of  chlorides  of 
silicon  collects  in  the  receiver.  If  the  tem- 
perature within  the  combustion  tube  was 
not  too  high,  two-thirds  of  this  is  silico- 
chloroform.  It  may  be  obtained  pure  by 
redistillation.  The  distilling  flask  must  not 
be  heated  with  the  naked  flame,  but  placed 
in  a  water-bath  kept  at  4O°-5o°.  Boiling 
point  of  silicochloroform,  37°-38°. 

HYDROGEN    PERSULPHIDE 

Sabatier,  Bl.  (2)  44,  169. 
Rebs,  A.  246,  356. 

Dissolve  40  grammes  potassium  hydrate 
in   125  c.c.  water,   saturate   with   hydrogen 


46     INORGANIC  CHEMICAL  PREPARATIONS 

sulphide,  and  boil  in  a  flask  with  sulphur  as 
long  as  any  dissolves.  Allow  to  stand  until 
clear,  and  pour  the  clear  solution  slowly 
into  an  ice-cold  mixture  of  60  c.c.  each 
hydrochloric  acid  (S.  G.  1.18)  and  water. 
Allow  to  stand  in  a  separating  funnel  sur- 
rounded by  ice  until  the  oil  settles.  Collect 
the  oil,  wash  it  with  ice  water,  and  dry  with 
filter  paper.  Distil  carefully  at  a  pressure 
of  40  to  80  mm.  Boiling-point  below  80°. 

BARIUM    OXIDE 

Fourcroy  &  Vauquelin,  A.  ch.  21,  277. 
Berthier,  A.  ch.  p.  22,  231. 

Put  2  kilos  heavyspar  and  500  grammes 
charcoal,  carefully  mixed,  into  a  Hessian 
crucible,  cover  with  a  layer  of  powdered 
charcoal,  and  heat  to  bright  redness  for  two 
hours.  When  cool  throw  into  cold  water 
and  add  slowly  dilute  nitric  acid,  avoiding 


HYDRATED  BARIUM  PEROXIDE  47 

much  excess  of  acid  (Hood).  When  all 
is  in,  heat  to  boiling,  filter  while  hot,  and 
evaporate  to  small  bulk.  Purify  the  barium 
nitrate  by  crystallization,  and  bring  it  little 
by  little  into  a  hot  porcelain  or  graphite 
crucible  coated  with  barium  sulphate.  Heat 
to  quiet  fusion,  put  the  crucible  into  a  tight 
iron  box  to  cool,  separate  the  core  from 
the  outer  layer,  break  it  up  and  keep  in 
tightly  stoppered  bottles. 

HYDRATED    BARIUM    PEROXIDE 

Th^nard,  A.  ch.  p.  8,  306. 
Boussingault,  C.  r.  32,  261. 
Thomsen,  B.  7,  73. 

Heat  barium  oxide  in  a  combustion  tube 
to  dull  redness,  and  pass  in  a  rapid  current 
of  moderately  dry  oxygen,  free  from  carbon 
dioxide,  as  long  as  any  is  absorbed.  Cool 
and  dissolve  in  the  calculated  quantity  of 


48     INORGANIC  CHEMICAL  PREPARATIONS 

ice-cold,  dilute  hydrochloric  acid.  Add  solu- 
tion of  barium  hydroxide  little  by  little 
until  the  precipitate  formed  is  perfectly 
white.  Then  filter,  and  to  the  filtrate  add 
baryta  water  to  complete  precipitation, 
avoiding,  however,  any  excess  of  barium 
hydroxide.  Wash  the  precipitate  with  ice 
water,  and  dry  on  clay  plates. 

HYDROGEN    DIOXIDE 

Thomsen,  B.  7,  73. 
Wolfenstein,  B.  27,  3307. 
Spring,  Z.  Anorg.  8,  424. 
Bruhl,  B.  28,  2853. 

Cool  a  mixture  of  50  c.c.  sulphuric  acid 
and  500  c.c.  water  with  ice  and  salt,  and 
add  slowly  hydrated  barium  peroxide  until 
almost  neutral.  Filter  and  add  more  perox- 
ide until  barium  chloride  no  longer  gives  a 
precipitate.  Test  for  barium  salts  with  sul- 


HYDROXYLAMINE  SULPHATE  49 

phuric  acid,  and  if  present  add  sulphuric 
acid.  By  thus  alternating  if  necessary  a 
solution  may  be  obtained  giving  no  test  for 
either  barium  or  sulphuric  acid.  Allow  to 
stand  in  the  refrigerator  for  a  day,  filter  and 
evaporate  on  the  water-bath  in  a  smooth 
platinum  or  porcelain  dish  until  the  liquid 
begins  to  decompose,  then  cool  rapidly,  and 
concentrate  further  by  distillation  in  vacuo. 

HYDROXYLAMINE   SULPHATE 

Divers,  Soc.  69,  1665. 

Dissolve  75  grammes  commercial  sodium 
nitrite  and  140  grammes  crystallized  sodium 
carbonate  in  as  little  ice  water  as  possible, 
and  lead  in  sulphur  dioxide  until  just  acid, 
agitating  thoroughly,  and  keeping  the  tem- 
perature 2°-3°  below  zero  by  immersing  in 
brine  and  ice.  Add  a  few  drops  of  sulphuric 
acid,  and  heat  very  slowly  to  between  90° 


50    INORGANIC  CHEMICAL  PREPARATIONS 

and  95°.  Keep  at  9O°-95°  for  about  two 
days,  or  until  all  the  sodium  oxamido-sul- 
phonate  has  been  hydrolyzed.  (To  deter- 
mine this  add  to  some  of  the  solution  an 
excess  of  barium  chloride,  filter,  add  to  the 
filtrate  some  potassium  chlorate,  and  boil 
for  a  few  minutes ;  if  no  precipitate  forms 
the  action  is  over.)  When  the  hydrolysis  is 
completed  neutralize  with  sodium  carbonate, 
using  methyl  orange  as  indicator ;  evaporate 
until  the  solution  weighs  800-825  grammes, 
and  cool  to  5°-8°  below  zero.  Separate 
from  the  sodium  sulphate,  and  evaporate 
until  the  solution  yields  at  the  ordinary  tem- 
perature abundant  crystals  of  hydroxylamine 
sulphate.  Powder  the  crystals  of  sodium  sul- 
phate which  first  separated,  wash  with  little  ice 
water,  and  add  washings  to  the  mother  liquor 
from  the  hydroxylamine  sulphate.  Work 
this  up  carefully.  Purify  the  crude  hydroxyl- 
amine sulphate  by  recrystallization.  Devise 


PHOSPHONIUM  IODIDE  51 

a  method  for  getting  hydroxylamine  chloride 
from  the  sulphate,  and  try  it. 


PHOSPHONIUM    IODIDE 

Baeyer,  A.  155,  269. 

Dry  carefully  100  grammes  phosphorus  in 
a  500  c.c.  tubulated  retort,  add  sufficient 
carbon  disulphide  to  dissolve  it,  and  then 
slowly  and  carefully  170  grammes  dry 
iodine,  keeping  the  whole  cold,  and  the 
apparatus  filled  with  carbon  dioxide.  Distil 
the  carbon  disulphide  very  slowly  in  a  water- 
bath  until  it  is  entirely  driven  off.  Allow  to 
cool,  and  by  means  of  a  long,  thin-walled 
glass  tube  connect  the  retort  with  a  receiver 
protected  by  a  drying  tube,  which  communi- 
cates with  the  outer  air  or  a  good  draught. 
Bring  a  drop  funnel  into  the  tubular,  and 
drop  in  very  slowly  60  grammes  water. 
Heat  until  no  more  phosphonium  iodide 


52     INORGANIC  CHEMICAL  PREPARATIONS 

comes  over,  or  until  it  no  longer  comes  over 
white.  Transfer  the  phosphonium  iodide, 
most  of  which  will  be  found  in  the  glass 
tube,  as  quickly  as  possible  to  tightly  stop- 
pered bottles.  The  apparatus  must  be  con- 
stantly full  of  carbon  dioxide. 


EXERCISES  53 

Make  three  or  four  of  the  following 
substances,  consulting  the  original  articles 
for  methods  of  preparation:  — 

Allotropic  Forms  of  Silver.  M.  Carey 
Lea,  Am.  J.  Sc.  (3)  37,  476. 

Ammonium  Peroxide.  Melikoff  and  Pis- 
sarjewsky,  B.  30,  3144;  Z.  Anorg.  18,  89. 

Calcium.     Moissan,  C.  r.  126,  1753. 
Chromium.     Moissan,  C.  r.  119,  185. 
Ferrotitanium.     Goldschmidt,  A.  301,  19. 

Hydrazoic  Acid.  W.  Wislicenus,  B. 
25,  2085. 

Hydroxylamine.  Lobrey  de  Bruijn,  Rec. 
II,  i £. 

Nickel  Carbonyl.  Mond,  Langer  & 
Quincke,  Soc.  57,  750. 

Potassium  Persulphate.  Marshall,  Soc. 
59,  772. 

Uranium.     Moissan,  A.  ch.  p.  (7)  9,  268. 


54    INORGANIC  CHEMICAL  PREPARATIONS 


TABLE   OF   SOLUBILITIES 

When  the  aqueous  solution  is  saturated  at  the  temperature 
indicated  it  contains  for  every  100  grammes  water  (X) 
grammes  salt  (calculated  in  every  case  as  anhydrous  salt) . 


TEMPERATURES  INDICATED. 

Zero. 

15°. 

100°. 

Ammonium  Carbonate  .... 
Ammonium  Chloride  .... 
Ammonium  Hydrogen  Carbonate 
Ammonium  Nitrate  
Ammonium  Sulphate  .... 

29 

12 

97 
7i 
3i 

10 

1.6 

5° 
0.17 
0.19 

IS 

36-5 

55 
5 
5 

100 

35 
18 
161 
75 
34-5 
20 

3-i 
3-3 
66 
0.16 

0.2 

8  to  9 

20 

75 

almost 
insol. 

very  sol. 
48 

67 
sol. 

65 

7 

10 

77 

97-5 
59 
90 

50 
3i 

155 
0.08 
0.17 

73 

127 
123 

53 

54 

100 

Barium  Dithionate  
Barium  Hydrate  

Boric  Acid  

Calcium  Chloride  
Calcium  Hydrate  
Calcium  Sulphate  . 

Chrome  Alum  

Cupric  Chloride 

Cuprous  Chloride  • 

lodic  Acid  

Lead  Nitrate  

Manganous  Chloride  .... 
Manganous  Dithionate  .... 
Manganous  Sulphate  .... 
Mercuric  Chloride  ..... 
Potassium  Bichromate  .... 

TABLE  OF  SOLUBILITIES*    '          ' 


^ 

TEMPERATURES  INDICATED. 

Zero. 

15°. 

100°. 

Potassium  Carbonate     .... 
Potassium  Chlorate  

90 

3-3 
28 

no 
6 
33 

156 
56 
56 

Potassium  Chloride  

Potassium  Fluortitanate      .     .     . 

0.5 

i 

— 

Pbtassium  Hydrogen  Sulphate     . 

36 

46 

121 

Potassium  Nitrate     

13 

26 

247 

Potassium  Nitrite      

— 

very  sol. 

— 

Potassium  Permanganate    . 
Potassium  Sulphate  

8.5 

1  20 

7 
35-6 
7 

6 
10.3 

almost 
insol. 
2OO 

I6.5 

35-8 
9 

26 

IOOO 

45-5 
39-8 

Silver  Hyponitrite     

Silver  Nitrate  . 

Sodium  Carbonate 

Sodium  Chloride  . 

Sodium  Hydrogen  Carbonate  .     . 

Sodium  Hydrogen  Phosphate 

2.5 

73 

5 
14 
i-5 

47 

6 
85 

very  sol. 

13 

2O 

4 
65 

99 

i  So 

42 
55 

Sodium  Nitrite     

Sodium  Tetraborate  

Sodium  Thiosulphate     .... 

Strontium  Chloride   
Strontium  Hydrate    .... 

44 
0.4 

Si 
0.66 

102 
21.8 

; 

The  figures  given  have  been  largely  taken  from  Comey's 
Dictionary  of  Chemical  Solubilities.  In  most  cases  fractions 
have  been  omitted.  Where  two  or  more  observers  give 
different  data,  an  average  has  generally  been  struck. 


INDEX 


Aluminium  Chloride,  40. 
Ammonium  Nitrate,  13. 
Ammonium  Sodium  Phosphate, 

13- 

Antimony  Oxychloride,  27. 
Antimony  Trichloride,  25. 
Arsenic  Acid,  15. 

Barium  Dithionate,  12. 

Barium  Oxide,  46. 

Barium  Peroxide,  hydrated,  47. 

Boric  Acid,  9. 

Boron,  10. 

Chromic  Anhydride,  16. 
Chromium   Potassium    Sulphate, 

15- 

Chromous  Acetate,  17. 
Cuprous  Chloride,  6. 

Fluorsilicic  Acid,  25. 

Hydriodic  Acid,  19. 
Hydrobromic  Acid,  18. 
Hydrogen  Dioxide,  48. 
Hydrogen  Persulphide,  45. 
Hydroxylamine  Sulphate,  49. 

lodic  Acid,  34. 
Iodine  Trichloride,  33. 

Lead  Dioxide,  7. 
Lead  Nitrite,  basic,  5. 


Manganese,  31. 
Manganous  Chloride,  31. 
Mercuric  Oxide,  8. 

Nitric  Anhydride,  37. 
Nitrogen  Iodide,  36. 
Nitrogen  Tetroxide,  36. 

Phosphonium  Iodide,  51. 
Phosphorus  Trichloride,  23. 
Potassium  Chlorate,  2. 
Potassium  Fluortitanate,  34. 
Potassium  Permanganate,  41. 

Silicochloroform,  43. 

Silicon,  42. 

Silver  Hyponitrite,  29. 

Silver  Nitrate,  27. 

Sodium  Ammonium   Phosphate, 

13- 

Sodium  Chloride,  I. 
Sodium  Hydrogen  Carbonate,  3. 
Sodium  Nitrite,  4. 
Sodium  Thiosulphate,  n. 
Strontium  Chloride,  30. 
Strontium  Hydroxide,  30. 
Sulphur  Monobromide,  35. 
Sulphuric  Anhydride,  39. 
Sulphuryl  Chloride,  22. 

Tin  Tetrachloride,  21. 
Titanic  Oxide,  35. 

Zinc  free  from  Arsenic,  14. 


57 


THE  PRACTICAL  METHODS 

OF 

ORGANIC  CHEMISTRY 

AUTHORIZED  TRANSLATION 
1 2 mo.    Cloth.    Price,  $1.60,  net 

BY  TRANSLATED  BY 

LUDWIG  GATTERMANN,  Ph.D.,         WILLIAM  SHAFER,  Ph.D., 

Professor  in  University  of  Heidelberg.         Instructor  in   Organic    Chemistr* 

in  Lehigh  University. 


THE  GUARDIAN. 

"The  selection  and  judgment  throughout  is  excellent.  The  book 
is  a  most  useful,  practical  adjunct  to  any  good  text-book  on  organic 
chemistry." 

PHARflACEUTICAL  REVIEW. 

'*  This  is  a  book  that  should  be  in  the  library  of  every  teacher  of 
organic  chemistry,  and  one  which  will  no  doubt  be  of  great  value 
to  students  in  their  second  year  of  organic  chemistry.  Its  chief  pecu- 
liarity and  merit  is  in  the  great  stress  laid  on  practical  laboratory  work. 
.  .  .  It  is  permanently  a  worker's  guide." 

NATURE. 

"  Since  the  advance  of  organic  chemistry  in  this  country  must,  in  a 
measure,  depend  on  the  nature  of  the  available  text -books,  both  the 
author  and  the  translator  deserve  our  thanks  for  providing  us  with 
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OUTLINES 

OF 

INDUSTRIAL  CHEMISTRY 

A  TEXT-BOOK  FOR  STUDENTS' 
By  FRANK    HALL   THORP,   Ph.D., 

Instructor  in  Industrial   Chemistry  in  the  Massachusetts  Institut 
of  Technology. 

Cloth.    8vo.    Price,  $3.50  net 


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Department  of  Chemistry,  Washington  and  Lee  University. 

"The  book  is  brought  thoroughly  up  to  date,  and  in  some  cases  the 
lines  of  probable  development  are  nicely  foreshadowed.  The  descrip- 
tions are  particularly  lucid  and  the  illustrations  well  selected. 

The  general  arrangement  and  make-up  of  the  book  is  excellent,  and 
. .  .  altogether  the  book  fills  well  a  need  long  felt  by  teachers  of  Indus- 
trial Chemistry. 

I  shall  adopt  the  book  for  my  class  and  shall  take  pleasure  in 
recommending  it." 

CHARLES  E.  COATES,  Jr.,  Ph.D., 

Professor  of  Chemistry,  Louisiana  State  University. 

"  I  have  examined  it  carefully  and  think  it  a  most  excellent  book, 
meeting  a  want  I  have  long  felt  in  my  higher  classes.  I  have  intro- 
duced it  in  this  year's  classes." 

W.   A.   NOYES,   in  Science. 

"  The  descriptions  of  processes,  while  necessarily  concise,  are  clear 
and  interesting.  The  author  has  evidently  made  a  careful  study  of 
recent  methods  of  manufacture  as  well  as  of  older,  standard  processes. 
The  frequent  reference  to  American  practice  is  an  important  feature 
which  distinguishes  the  book  from  other  works  on  chemical  technology. 
A  select  bibliography  follows  each  subject,  and  will  he  found  very 
useful." 


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